CN201012323Y

CN201012323Y - Sodium particle preparation device

Info

Publication number: CN201012323Y
Application number: CNU2006201728159U
Authority: CN
Inventors: 赵洪滨; 姬忠礼; 袁桂梅
Original assignee: China University of Petroleum Beijing
Current assignee: China University of Petroleum Beijing
Priority date: 2006-12-29
Filing date: 2006-12-29
Publication date: 2008-01-30
Anticipated expiration: 2016-12-29

Abstract

The utility model provides a sodium particle preparation device, which includes a reaction kettle provided with an agitator mechanism and a baffle inner member, and is characterized in that the agitation shaft of the agitation mechanism is longitudinally provided with a three-layer open-type turbine agitator, wherein The blades of the upper and lower agitators are hinged, and the inclination direction of the blades is set so that the upper agitator and the lower agitator can realize the effect of pressing down and turning up the materials respectively during stirring and moving along the axial direction. The middle agitator The blades are straight blades; the internal components of the baffles include 2 to 4 layers of baffles arranged in a staggered manner on the inner wall of the reactor, and each layer includes 3 to 5 baffles arranged at intervals to form an inner baffle. There is a distance between the baffle plate of the component and the inner wall of the kettle. The device of the utility model is especially suitable for the production process of synthesizing triphenylphosphine by the sodium method, which is beneficial to ensure the complete reaction of metal sodium at a relatively low stirring speed, and at the same time ensures the safety in industrial production.

Description

Sodium particle preparation device

Technical field

The utility model is the device that can realize height of materials dispersion and shearing about a kind of, especially about a kind of sodium particle preparation device.

Background technology

The mechanical agitation reactor is to implement mixing of materials to promote one of important form of heat transfer, mass transfer.The structure of mechanical stirring kettle comprises agitator structure and baffle arrangement.In order to improve the performance that mixes to material, at different technology, need optimize targetedly the structure of inner member (baffle plate) and agitator, that is, standard baffle plate and standard impeller structure may not necessarily satisfy specific technological requirement.

The a lot of employing in the synthesis technique of sodium metal as raw material, that guarantees sodium metal and other reaction raw materials fully contacts realization response often fully and improve the key of reaction yield, generally all need earlier the sodium metal grain to be disperseed to become powder sodium, for example, adopting the sodium legal system to be equipped with in the production technology of triphenylphosphine, be to adopt sodium metal, chlorobenzene and phosphorus trichloride are the synthetic triphenylphosphine of raw material, sodium metal is generally the sodium grain, abundant and effective contact the with chlorobenzene in reaction is one of key that reacts completely, become particle diameter less than 70 microns high-specific surface area particulate so need that earlier sodium metal is carried out decentralized system, if the particle of sodium metal is bigger than normal in the reaction, carrying out along with reaction, sodium phenide that particle surface can be formed gradually and sodium chloride cover, reduced the contact area of sodium metal and chlorobenzene, cause reaction not exclusively, and, because the existence of unreacted metal sodium has also increased the unsafe factor of postprocessing working procedures.In this class synthesis technique, for the sodium grain of high-ratio surface is provided, utilize present reactor, even under the effect of agitator and inner member, also need material is implemented high-speed stirred, speed of agitator need be brought up to 350～2000 rev/mins.For the large-volume reaction kettle of using in the suitability for industrialized production, so high mixing speed has very high requirement for the structure of reactor, and keep high rotating speed operation aborning security is also proposed higher requirement.

The agitating device that is used for reactor has aerofoil profile slurry formula to stir or the turbine type stirring usually, also can be their combination (two layers of combination), and inner member is generally positioned vertical in the still internal face, i.e. wall baffle plate, commonly four baffle plates of still inwall symmetry installation.But the various combination mode of agitator structure and baffle arrangement can produce very big-difference for the mixing effect of material.For the impeller under the off-rating, baffle plate machine Study of Interaction also is the important component part of technical study.The high degree of dispersion of sodium metal is realized the preparation of powder sodium (sodium grain) having its particularity, also do not have particular study and report at present at the reactor structure of this technology.

The utility model content

The technical problem that the utility model solved provides a kind of reaction unit that is applicable to the preparation of sodium grain, it is sodium particle preparation device, by structural improvement, realize that material is than efficient mixing and shear effect under the slow-speed of revolution, the security that improves production process simultaneously to agitator and inner member.

The utility model solves above-mentioned technical problem by following technological means:

A kind of sodium particle preparation device, it is the reactor that is provided with stirrer mechanism and baffle plate inner member, the shaft of described agitator is vertically arranged with three layers of open-type turbine stirrer, the blade of the upper and lower agitator wherein is a hinging type, the incline direction of blade be configured such that upper strata agitator and lower floor agitator are implemented to press down to material respectively in realizing stirring and on turn over and the effect of motion vertically, the blade of middle level agitator is straight leaf formula; Described baffle plate inner member comprises 2～4 layers of hydraulic barrier that are arranged at the reactor inwall with the stagger arrangement formula, and every layer comprises 3～5 baffle plates that are provided with at interval, between the baffle plate of composition baffle plate inner member and the inner wall of kettle spacing is arranged.

As industrial production device, the stainless steel cauldron that the described reactor preferable volume of the sodium particle preparation device that the utility model provides is 100～3000 liters, reactor ratio of height to diameter 1: 1～1: 1.6, and the ratio of reactor internal diameter and stirrer diameter 2.5: 1～4.5: 1; The horizontal direction that is arranged on of baffle plate inner member is in stirring region substantially, the space internal diameter that the baffle plate inner member surrounds in still is 0.8～0.9: 1 with kettle internal diameter ratio, baffle plate and the spacing between the inner wall of kettle of forming the baffle plate inner member are 0.01～0.02: 1 with still internal diameter ratio, and described baffle plate is for radially to be 10 °～30 ° settings with the still endosome, be provided with towards with the rotation direction contrary of agitator.

Utilize this synthesis reaction vessel, setting and combination by stirring vane, stirring at the middle and upper levels, hinged joint makes material motion down vertically, lower floor's hinged joint then makes material move vertically, axially the effect that mixes is significantly strengthened, and straight leaf (also claiming flat leaf) is stirred simultaneously to material generation shear action in the middle level, cooperate baffle plate from the oblique setting of wall, material drives current downflow at stirring vane, also be subjected to simultaneously the shearing of baffle plate, thereby material can fully be mixed and efficient the shearing, especially be beneficial to the sodium grain that obtains having high-specific surface area.

According to sodium particle preparation device of the present utility model, be respectively equipped with 3 blades on the wheel hub of described three layers of open-type turbine stirrer, the hinging type blade of the upper and lower turbine stirrer is respectively 0.2～0.3 in the standoff height of vertical plane and the ratio of stirrer diameter.

Preferably, 2～4 layers of hydraulic barrier inner member total height that are arranged at the reactor inwall are 0.35～0.65 of still endosome height.

For the benefit of to the axial mixing of material, the lower surface of the upper surface of upper strata mixing arm and lower floor's mixing arm vertically is formed with an inclined-plane along blade, and this inclined-plane is near the downward-sloping side of blade, and surface width is no more than 1/3 of width of blade.

In a specific embodiment of the present utility model, be respectively equipped with 3 blades on the wheel hub of described three layers of open-type turbine stirrer, vane thickness 5.0～10.0mm, width of blade 80～100mm, the diameter 60～120mm of shaft;

Described hydraulic barrier inner member is made up of 3 layers of baffle plate, and every layer has 4 baffle plates and equidistantly is fixed on inner wall of kettle;

More preferably, the reactor of described sodium particle preparation device is the stainless steel cauldron of 100～2000 liters of volumes, reactor ratio of height to diameter 1: 1.2～1: 1.4; The baffle plate of the reactor inwall setting vertically ratio of height and kettle height is 1: 6～1: 8, baffle plate thickness 5.0～10.0mm, and every baffle plate is 0.05～0.1 of a kettle internal diameter along the radial width of still endosome.

Device of the present utility model can be widely used in sodium and be used for the production technology of many products of synthetic fine chemicals as raw material, and all is favourable for enhancing productivity.Concrete operations are dispersed into the sodium sand of high-specific surface area as decentralized medium with sodium for the solvent (for example alkylbenzene and alkane) that adopts boiling point and be higher than sodium fusion point, then according to the needs of the different synthesis techniques process with replacing dispersion medium.Production technology with the synthetic triphenylphosphine of sodium method is an example, adopt device of the present utility model, sodium metal adds in the toluene, under of the effect of this reactor through described three layers of agitator and hydraulic barrier inner member, the rotating speed that control ratio is lower can be realized effectively shearing and disperseing, become particle diameter less than 70 microns sodium grain, because the high-specific surface area of sodium grain, the contact area of sodium metal and chlorobenzene can significantly increase, be beneficial to the complete reaction of sodium metal, no matter be security aspect, all have positive meaning from production cost and post processing.

Description of drawings

Fig. 1 is the whole interior structural representation of an example of the utility model sodium particle preparation device (powder sodium synthesis reactor).

Fig. 2 is the schematic cross-section of the internal structure of reactor among Fig. 1.

Fig. 3 A, Fig. 3 B, Fig. 3 C are respectively the structural representation that Fig. 1 provides the projection of upper, middle and lower layer stirring vane on vertical plane in the reactor, and Fig. 3 A ', Fig. 3 B ', Fig. 3 C ' are respectively the schematic top plan view of the stirring vane among Fig. 3 A, Fig. 3 B, Fig. 3 C.

The expansion schematic diagram of the reaction kettle body that Fig. 4 provides for Fig. 1 has wherein shown the set-up mode of inner member baffle plate at the still inwall.

Fig. 5 A, Fig. 5 B, Fig. 5 C are respectively the sectional schematic diagram of the upper, middle and lower layer blade that agitator is set in the utility model stirred autoclave.

The specific embodiment

Further specify embodiment of the present utility model below in conjunction with accompanying drawing,, do not limit but practical range of the present utility model is not constituted so that the reader can understand design philosophy of the present utility model and flesh and blood more accurately.

Consult shown in Figure 1, reactor 1 is 500～2000 liters of stainless steel cauldrons, an open-type turbine agitator 2 that three-decker is vertically arranged is set in the still, inner wall of kettle is provided with three layers of hydraulic barrier inner member 3 in the stagger arrangement mode, and baffle plate inner member 3 setting in height is located substantially on the stirring region of agitator 2.

The set-up mode of hydraulic barrier inner member 3 can be simultaneously referring to Fig. 2 and Fig. 4, equidistantly distributes for three layers by 12 baffle plates 31 minutes, and be that stagger arrangement is arranged in vertical direction between 4 baffle plates of each layer.Baffle plate 31 is fixed on the still inwall by the stainless steel projection 32 that is welded on the rear portion in advance, and a spacing b is arranged between baffle plate 31 and the inner wall of kettle ₀, be beneficial to material flowing in stirring.Baffle plate 31 radially is an angle θ with the still endosome and is provided with, and baffle plate 31 be obliquely installed towards with the direction of rotation of agitator 2 (among Fig. 2 shown in the arrow) contrary, be beneficial to when material is mixed and be sheared.

Turbine agitator 2 vertically substantially equidistantly be provided with three layers of open-type turbine stirring, the wheel hub of every layer of stirring all has 3 stirring vanes 21, wherein the blade of the upper and lower stirring is a hinging type, all horizontal by an angle setting, the blade that stir in the middle level is straight leaf, please in conjunction with referring to Fig. 3 A, Fig. 3 A ', Fig. 3 B, Fig. 3 B ', Fig. 3 C, the schematic construction of the stirring vane shown in Fig. 3 C ', and Fig. 5 A, Fig. 5 B, Fig. 5 C displaying contents, the angle that is provided with of the blade that stir on the upper strata makes progress for the side along direction of rotation (stirring rotation direction), the angle that is provided with of lower leave is downward along the side of direction of rotation, and the blade that stir in the middle level is then for being horizontally disposed with.Like this, when agitator 2 rotates material enforcement stirring, (solid arrow represents to stir rotation direction as signal among Fig. 5 A, Fig. 5 B, Fig. 5 C, dotted arrow is represented the action direction to material) the upper strata blade can press down material, lower leave can will turn on the material, material can be realized axial mixing simultaneously, and the middle level blade is then sheared material.For improving mixing effect and strengthening axially mixing, the lower surface of upper strata blade and the upper surface of lower leave vertically are formed with an inclined-plane 22 respectively along blade, this inclined-plane 22 is near the downward-sloping side of blade, be beneficial in whipping process material is transmitted to the center of stirring region, cooperate the setting of baffle plate inner member, more improve shear effect, inclined-plane 22 width are approximately 1/3 of width of blade.

The structural parameters of this reactor are as follows:

The ratio of height to diameter H of reactor endosome: D=1: 1～1: 1.6, preferred 1: 1.2～1: 1.4;

The space inside diameter D that baffle plate surrounds ₀With the ratio of kettle inside diameter D be: D ₀: D=0.8: 1～0.9: 1;

Reactor internal diameter and agitator 2 diameters (that is, agitator rotates the diameter that forms border circular areas at horizontal plane) are than D: d _M=2.5: 1～4.5: 1; The diameter d of shaft _N=60～120mm, the width B of stirring vane 21 in every layer _x=80～100mm, stirring vane 21 thickness b ₂=5.0～10.0mm, the upper and lower hinged joint 21 are obliquely installed the standoff height b of back at vertical plane ₁With agitator 2 diameter d _MRatio b ₁/ d _M=0.20～0.30;

The baffle plate 31 vertical height h that the reactor inwall is provided with and the ratio h/H=1 of kettle height H: 6～1: 8, the horizontal width h of every baffle plate 31 ₀=0.05D～0.1D, baffle plate thickness b _h=5.0～10.0mm, baffle plate 31 and still endosome angle θ=10 between radially °～30 °, the distance between baffle plate and inner wall of kettle with the ratio of kettle inside diameter D is: b ₀: D=0.01～0.02: 1, every baffle plate is fixed on inner wall of kettle (quantity of this projection can be determined according to height of baffle plate) by two stainless steel projections 32, and two bump pitch x are defined as x: h=1: 3～1: 5.

Adopt above-mentioned stirred autoclave, dispersion at sodium metal prepares in powder sodium and the corresponding synthetic reaction process, mixing speed can be controlled at and be lower than 220 rev/mins, needn't operate under high rotating speed, guarantees obtaining the security that satisfactory powder sodium also is beneficial in the suitability for industrialized production simultaneously.

Claims

1. a kind of sodium particle preparation device, it comprises the reactor that is provided with agitator and baffle plate inner member, it is characterized in that, the agitator shaft of described agitator is longitudinally provided with three layers of open-type turbine agitators, wherein upper floor and lower floor are stirred The blades of the mixer are hinged, and the inclination direction of the blades is set so that the upper layer agitator and the lower layer agitator can realize the effect of pressing down and turning up the materials respectively during the stirring and moving along the axial direction, and the blades of the middle layer agitator are straight blades. The internal components of the baffles include 2 to 4 layers of baffles arranged in a staggered manner on the inner wall of the reactor, and each layer includes 3 to 5 baffles arranged at intervals to form the baffles of the internal components of the baffles and There is a distance between the inner walls of the kettle.

2. sodium particle preparation device according to claim 1, is characterized in that, this reactor is the stainless steel reactor of volume 100～3000 liters, and reactor aspect ratio is 1: 1～1: 1.6, and reactor internal diameter and The ratio of the diameter of the agitator is 2.5:1~4.5:1; the internal components of the baffle are arranged in the horizontal direction and are basically in the stirring area, and the ratio of the inner diameter of the space enclosed by the internal components of the baffle to the inner diameter of the reactor is 0.8:1~0.9 : 1, the distance between the baffle plate and the internal wall of the reactor and the inner diameter of the reactor are 0.01:1 to 0.02:1, and the baffle is 10° to the radial direction of the reactor inner body. 30° setting, the setting direction is opposite to the running direction of the agitator.

3. according to claim 1 and 2 described sodium particle preparation devices, it is characterized in that, the hub of described three-layer turbine agitator is respectively provided with 3 blades, and the hinged blade of upper floor and lower floor turbine agitator is in vertical The ratio of the projected height of the surface to the diameter of the stirrer is 0.2-0.3 respectively.

4. sodium particle preparation device according to claim 1, is characterized in that, the upper surface of upper floor agitator leaflet and the lower surface of lower floor agitator leaflet form an inclined plane longitudinally along blade, and this inclined plane is inclined downwards near blade On the sides, the width of the bevel does not exceed 1/3 of the width of the blade.

5. The sodium particle preparation device according to claim 1 or 2, characterized in that, the hub of the three-layer turbine agitator is respectively provided with 3 blades, the thickness of the blade is 5.0～10.0mm, and the width of the blade is 80～100mm. The diameter of the stirring shaft is 60-120mm.

6. The sodium particle preparation device according to claim 1, characterized in that, the total height of the internal components of 2 to 4 layers of baffles arranged on the inner wall of the reaction kettle is 0.35 to 0.65 of the height of the inner body of the kettle.

7. The sodium particle preparation device according to claim 6, wherein the internal member of the baffle is composed of 3 layers of baffles, each layer has 4 baffles and is fixed on the inner wall of the kettle at equal intervals.

8. The sodium particle preparation device according to claim 2 or 6, characterized in that, the reactor is a stainless steel reactor with a volume of 100 to 2000 liters, and the aspect ratio of the reactor is 1: 1.2 to 1: 1.4; The ratio of the vertical height of the set baffle to the height of the kettle body is 1:6 to 1:8, the thickness of the baffle is 5.0 to 10.0 mm, and the width of each baffle along the inner radial direction of the kettle is 0.05 to 0.1 of the inner diameter of the kettle.